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July 10, 1 .923. 1,461,539

E. MALLINCKRODT, JR

METHOD OF PURIFYING AND PACKAGING ETHER Filed March 18 1921 'asamefer' Fury/ed Ef/7er Tami W m 42) #18 i7 0/1/7035.

Patented July Ml T9233.

entree" stares EDWARD MALLINCKRODT, JR, 01E ST. LOUIS. MISSOURI, ASSIGNOR TO MALLTNC 1:1 0") attain PATENT creme,

' CHCAL WOR, 01? ST. LOUIS, MISSOURI, A CORPORATION 01E MISSOURI.

METHOD OE PURIEYING, AND JPACGING ETHER.

I Application filed March 18, 1921. Serial No. 453,285.

To all whom it may concern:

Be it known that I, EDWARD MALLINo- KRODT, J r., a citizen of the United States, residing at the city of St. Louis and State of Missouri, have invented a new and useful Method of Purifying and Packaging Ether, of which the following is a specification.

The object of this inventioinis to provide a novel and effective method, or plan of procedure, for purifying and packaging the highest grade of ether for anaesthesia and other purposes where absolute freedom from the slightest tendency to alteration in storage is desirable. To attain this end it is necessary to produce ether free from oxygen and to package the same without the access of air. The invention, therefore, relates to a method of producing and packaging air-free ether in hermetically sealed cans without the access of air.

My invention may be practiced by use of any appropriate means or apparatus for excluding air from the containers in which the ether is to be placed, and by placing theair-free purified ether in the containers while the air is excluded from both the containers and the ether, and then hermetically closing and sealing the containers so that the air will be permanently excluded therefrom.

In the accompanying drawings- Fig. 1 is a view, diagrammatic in nature,

of an apparatus for practicing the invention.

Fig. 2 is a sectional view showing anappropriate arrangement of the device for applying a cap or closure to the can or contamer in which the air-free purified ether is to be packaged.

Fig. 3 is a view showing an appropriate arrangement for securing the cap or closure to the container.

The apparatus which is shown is one form of usable apparatus for practicing the invention, though it will be understood that the invention may be practiced in any other form of apparatus capable of use to obtain the desired results. Accordingly, in describing generally the illustrated apparatus, I do not, to any extent, restrict or confine myself to the use of any definite or specific type of mechanism or apparatus.

As shown, the distillation column is provided with proper equipment of dephlegmator and condenser, and is set up in such a -mam1er that when a supply of ether is continuously fed in toward the middle of the column, the air-free purified ether flows from the bottom of the column into an airfree storage tank while the condenser is arranged to allow the escape of air and the removal of a small amount of'im ure ether. The ether may be fed into the istillation column continuously through an inlet pipe communicating with an elevated ether storage tank (provided with a fioat box equipment for maintaining a constant level), or in gaseous form from the stills in which it is manufactured, the essential feature being that the ether be subjected to a distillation or boiling out process in the distillation column in order to obtain an air-free urified condition of the ether.

,The et er is prevented from leaving the distillation column by the familiar action of the dephlegmator, which is similar to to those employed in the distillation industry. The result is that the ether vapors are condensed and a downward flow of liquid over the trays in the distillation column is produced. The air does not dissolve in the hot liquid and is carried out and eliminated by that portion of the vapors which pass into the condenser. By the time the main flow of ether has passed to the bottom of the distillation column it is free from air.

From the distillation column, the ether passes through an outlet pipe leading to a purified ether storage tank which is provided with a gasometer. The entire ap paratus is filled with pure nitrogen er other suitable protecting gas free of oxygen.

From the purified ether storage tank the ether is delivered in the purified air-free condition into the cans or containers inside a filling boxvfrom which the air has been displaced by pure nitrogen or other suitable protecting gas. The caps or closures are 'then placed on the cans and are securely Bllt) very high vacuum are difficult to maintain in operative condition, an ordinary vacuum pump is used and the air in the reservoir 1 is reduced to a satisfactory minimum by exhausting the air therefrom, and breaking the vacuum with nitrogen, and repeating the operation several times. The gasometer-is also in communication with the filling box through .a pipe 7, so that said filling box' is kept filled with the gas which is free of oxygen, it being understood that the filling box is free of air so that when the cans are delivered into the filling box they remain free of air.

The cans having been dropped into the filling box from the reservoir 1 are now successively moved by hand as hereinafter stated, or otherwise as desired, to the various positions of filling, capping, etc.,'dur ing all of which operations, the air is excluded from the filling box and therefore from the cans and from the ether that is placed in the cans. The cans are first filled with ether by means of a simple measuring apparatus seen at 8 in the pipe leading from the purified other storage tank into the filling box and arranged to discharge the required amount into the cans as they are moved successively into filling position Next the cans are moved from position A to position B, in which caps or closures are applied to the cans successively by a manually operated suction tube 9 extending through one wall of the filling box and being operative for the purpose of applying thesecaps or closures to the cans. After the caps or closures have been applied to the cans, the cans are moved successively. to a position C in which the closure fastening means 10 operates to crimp or secure the caps or air tight closures to the cans. Instead of a mechanical device such as illustrated at 10, the caps or closures may be soldered on while the cans are in the filling box. Such manipulation may be effected, if desired, by means of an appropriate soldering device, and by enclosing the hand in a rubber glove 11 having its sleeve portion hermetically connected with the wall of'the filling box around a suitable opening to permit the hand to be passed into the glove to operate the soldering, device. The cans may also be moved to the-various positions of filling. capping, etc., by use of the hand in the glove 11, the elasticity and flexibility of which permit the necessary movements-of the hand. The suction tube 9, as shown in Fig. 2, is mounted in a universal bearing joint to permit freedom of movement in every direction. As stated, the tube 9 is a suction tube and the caps may be picked up successively by touching the end of the tube to the caps contained in any support holding them. After a cap has been applied to the end of the suction tube 9, said tube is operated to deposit the cap on the nozzle of the can. I

that the filling box and the cans be freed from air and refilled with the protecting gas and that the ether also be free from air during the filling and sealing operations. No specific mechanism is shown for moving the cans to their various positions in the filling box, since it is obvious that their movement may be effected manually or me-- chanically.

'From the foregoing it. is apparent that my invention is complete in that it provides an efiicient and comparatively simplemeth- 0d or plan of procedure for sealing air-free purifiedether hermetically in air-free cans or containers, and this result is obtained by filling the cans with ether in a filling box or receptacle from which the air has been excluded and from which the air remains excluded during the entire operation. I do not restrict myself to unessential features of the invention, or to the specific way and arrangement shown, except as set forth in the appended claims] What I. claim and desire Letters Patent, is

1. The method of packaging ether in conta ners, which consists in placing the contalners in a substantial vacuum; passing the to secure by containers from. the substantial vacuum into a filling box; filling the containers with ether; and hermetically closing the containers and maintaininganatmosphere of gas containing no free oxygen in the box during the filling and closing steps.

2.- The method of preparing and packaging ether which consists in establishing a vacuum about and within the containers,

then establishing an atmosphere of gas con-- its taining no free oxygen, then removing all ,air from a body of ether, filling the con- 'talners with the air-free ether, hermetically neenaae closing the containers and maintaining the atmosphere of gas containing no free oxygen during the filling and closing steps.

3. The method of preparing and packaging ether which consists in placing containers in a closed chamber, exhausting the air from the chamber, removing the containers to a second chamber, removing all air from a body of ether, filling the containers with the air-free ether, hermetically closing the containers and maintaining an atmosphere of gas containing no free oxygen in the second chamber during the filling and closing steps.

4. The method which consists in establishing a vacuum about and within containers to be filled with ether, then establishing an atmosphere of gas containing no free oxy-v gen about and within said containers, filling said containers with ether and sealing said containers and maintaining the atmosphere of gas containing no free oxygen about said containers during the filling and closing steps.

5. The method which consists in removing the air from about and within containers to be filled with ether, then establishing an atmosphere of gas containing no free oxygen about and within said containers, filling said containers with ether and sealing said containers, and maintaining the atmosphere of gas containing no free ox gen about said containers during the fillmg and closing steps.

6. The method which consists in establishing a vacuum about and Within containers to be filled with ether, then establishing an atmosphere of gas containing no free oxygen about and withln said containers, filling said containers with air-free ether and sealing said containers and maintaining the afinosphere of gas containing no free oxygen about said containers during the filling and closing steps.

7. he method which consists in removing the air from about and within containers to be filled with ether, then establishing an atmosphere of gas containing no free oxygen about and within said containers, filling sa'd containers with air-free ether and sealing said containers and maintaining the atmosphere of gas containing no free oxygen about said containers during the filling and closing steps.

EDWARD MALLINCKRODT, Jn. 

